Method of refining wool-grease.



p of the outrun JAMES B. HANBY AND ROBERT ISI-EAIK, GE? PITTSBUEZ'GH, PENNfiYLVANIAt, ASSIGN- OBS 'I'O PITTSBURGH TESTING- LABURATQRY, G13 PITTSBURGH, PENHS15LVJEiNJCA, A.

COR'EOBATIGN O1? PEHEQ SYLVANIA.

actose.

1% Drawing.

To all whom it may concern I Be it known that we, James O. HANDY andRonsie'r M. lsnAM, both citizens the United States, residing at Pittsburgh, Allegheny county, Pennsylvania, have invented a new and useful Method of Refining Nooh Grease, of which the following is a full, clear, and exact description. 4

Our invention has relation to an improved 'method ofrefining wool grease to obtain what is known as neutral WOOl grease or lanolin. These products are used largely in the leather industry, the lubricating oil. industry, and in pharmacy.

The wool grease available for our method of treatment is of two kinds, namely: naphthe extracted greasev obtained by treatment raw Wool With naphtha, and brown Wool grease, or degras, obtained by acidification of the soapy water obtained in the usual processes of wool scouring.

The naphtha extracted grease is of a lighter color and contains less. free fatty acids, while the other product" contains all the fatty acids which were in the soap. Our method of refining is applicable to both these products, although we preferably use the naphtha extracted grease.

The refinin problem. consists in the removal of the Iree fatty acids, together with a small portion of the neutral grease, to produce a: product which bleaches readily to a yellow" color, is neutral and WlllCl1-COI1SlSl3S chiefly of the Waxy portion of the original grease. This problem is a diiiicult one, be cause of. the tendency of the grease when stirredwith watery liquids toform a resise tant emulsion therewith.

It has been usual in the prior art to first neutralize or saponify the greaseby the "use oi an alkali (soda or potash) in an amount slightly in excess of the quantity required to combine with the free fatty acids. The next step'has been the separation of the soap thus produced from the neutral wool grease which it is desired to recover. Ifthc mixture is placed in Water, or if Water is added to the mixture and the mass is stirred, an

emulsion will be formed even before all the soap is dissolved. The solution of the soap 1s alsohindered by the stitlconsistency of the wool grease itself.

Ourlhvention provides a method by which the objectionable emulsificat on referred to Specification of Letters Patent.

Application filed April 22, 1551 grease to be refined is first austic soda in water solusuitable lieu 11 also contains a small bleaching.

Patented (lot Serial l fe. 353,52412,

.io', was.

is obviated and by means of which a satis factory product can be economically produced on a commercial scale.

in accordance with our invention the wool heated with about per cent. of 7 tion, in a steam-jacketed kettle, r by other "ig means. The mixture is stirred until testing shows that there is no longer any free alkali; The mixture of soap and unsaponified wool grease thus produced is made resistantto subsequent emulsiiication and more easily washed free from soap by the addition at this stage of about six gallons of petrolic ether or naphtha or gasolene for each one hundred pounds of grease. Preferably the mass is allowed to cool to a temperature of approximately 100 degrees Fahrenheit before this solvent is added. The mixture is then poured upon the surface of approximately five times its volume of Water, thewater preferably havmg a temperature between degrees and degrees Centigrade. At this stage the grease nurture should not be stirred with water, but'may be moved cautiously, so as to permit the solution of a considerable until the greater part of the soap is removed.

A warm salt solution, preferably about a 2 per cent. solution. is then run in and is agitated with the grease, until all but a very small annum'nt.oi. the .soap has been washed out. The removal oifthe soap may be hastened by using weal "alt solutions instead of water previougjto he running" in of the nal salt solution, since this further increases the resistance to emulsification. The remainin soap is then decomposed by the use of a small amount of calcium 'chlorid solution. At this stage, the grease has ab; sorbed a considerable "amount of Water, although it has not formed an emulsion. It-

' amount of lime soap. must therefore be dried before The grease The water is preferably eliminated by adding petrolic ether, and distilling up toa temperature Where the water passes over with, the solvent-. Thegrease is theh cooled and is ready for bleaching. This bleaching may be carried out by any known method.

lVe prefer, however, -to employ the method which is des ribed and claimed in the copending application of James 0. Handy, one

of the applicants herein, Serial No. 92,845, filed April 22, 1916. In accordance with that method the grease is dissolved in petrolic ether and is agitated with fullers earth. By this method we secure a bleaching effect which it isimpossible to obtain by treatment of the grease alone with fullers earth. Instead of disposing of the water by distillation of the wet grease before bleaching, the grease may be dried by adding sufficient fullers earth to absorb the water, and then heating in pans in a drying oven at a temperature of from 100 degrees to 110 de-- grees centigrade. The dry material is then agitated with petrolic ether and filtered.'

In either case the grease may be recovered from the petrolic ether solution by distilling ofi the solvent in a suitable form of stillpreferably a still having a closed steam coil and a condensing attachment. The petrolic ether is then ready for further use.-

The recovered grease may be freed from petroleum odors by blowing it with air or other suitable gas at a temperature of from 90 degrees torlOO degrees C.

The product produced is a highly satisfactory one, being perfectly neutral,.is of the desired yellow color when bleached, and

- the different steps thereof and in the dilfercut temperatures named, without departing from the spirit and scope of our invention as defined in the appended claims.

By the term petrolic ether as used herein and in the appended claims, we intend toinelude naphtha, -gasolene, and allsimilar pe-- troleum products having a ,sufliciently low boiling point. The boiling point should not be, sufiiciently low to'ca'use losses, and, on the other hand, it shouldnot be sufiiciently high to give undesirable residual products under the conditions of evaporation employed. In practice we have found a boiling point of from degfiees to 100 degrees (3., and preferably between 80 degrees and 100 degrees (3., to give good results.

' We claim:

1. In the art of refining wpol grease, the improvement whichconmsts 1n sapomfymg the free fatty acids in the grease, then preventing emulsifaation by adding petrol c ether tothe mixture of. soap and unsapomtied wool grease before attemptingto separate from each other the soap and the unsaponified wool grease, and then separating the soap from the unsaponified wool grease, substantially as described. I

2. .In theart of refining wool grease, the

method which consists in saponifying the free fatty'acids in the grease, permitting the mixture of soap and unsaponified wool grease to partially cool, then before attempting to separate from-each other the soap and unsaponified wool grease adding thereto a solvent which renders the mixture more resistant to subsequent emulsification and more easily freed from its soap, and then sep: rating the soap from the unsaponified wool grease-by means of an aqueousliquid,

substantially as described.

3. In the art of refining wool grease, the method which consists in saponifying the free fatty acids in the grease, permitting the mixture of soap and unsaponif ed wool grease to partially cool, then before atte1npt-' ing to separate from each other the soap and the unsaponified wool grease adding thereto a solvent which renders the mixture more resistant to subsequent emulsification and more easily freed from its soap, and then separating the soap from the unsaponified'.

wool grease by means of an aqueous liquid, substantially as descrlbed.

4. In the art of refining wool grease, the

method which consists in saponifying the free fatty acids in the grease, then preventing emulsification-by adding petrolic ether to the mixture of soap and unsaponified grease before attempting to separate from each other the soap and the unsaponified wool grease, and then washing the mixture free from soap, substantially as described.

5. Inthe art of refining wool grease, the method which consists in saponifying the free fatty acids in the grease, then preventing emulsification by adding petrolic ether to the mixture of soap and unsaponified grease before attempting to separate from each other the soap and the unsaponified wool grease, and then washingthe mixture free from soap by the use-of a weak sal solution, substantially as described.

6. In the art of refining wool grease, the method which consists in saponifying the free fatty acids in the grease, then preventing emulsification by adding petrolic ether 7. In the art of refining wool grease, the

method which consists in treating the grease 'to produce a mixture of soapand unsaponified wool grease, then rendering this mix ture resistant to subsequent emulsification' before attempting to separate from each other the soap and the unsaponified Wool grease, and then Washing the soap from the mixture by means of an aqueoushqu d, sub-.

ponified grease, then adding petrolic ether to this mixture, then pouring the mixture upon the surface of a volume of water to permit the solution of a part of the intermixed soap, and then removing [the water and agitating the mixture with a weak salt solution, substantially as described.

10, In the art of refining wool grease, the method which consists in treating the grease to produce a mixture-oiv soap and unsaponified grease, then adding petrolic ether to this mixture, then pouring the mixture upon the surface of a volume of water to permit tl'ie'solution of "a part of the intermixed soap, and then removing the water and agitating the mixture ,with a weak salt solution and decomposing the remainder of the soap by a substantially as described. e

11.. la the art of refining wool grease, the method. which consists in treating the grease to produce a mixture of, soap and unsaponiether before attempting to separate from each other the soap and the unsaponified wool grease, then removing the soap from the mixture, and then eliminating the water absorbed by the grease during the removal of the soap by adding a solvent and distilling at a temperature at which the Water will pass over With the solvent, substantially as described.

12. In the art of refining wool grease, the

calcium chlorid solution,-

a grease, then adding thereto petrolic f method which consists in treating the grease to produce a mixture ofsoap and unsaponified grease, then adding there-to petrolic ether before attempting to separate 'from' each other the soap and theunsaponiliedwool grease, then removing the soap from the mixture, and then eliminating the water ab sorbed by the grease during the removalof the soap by adding petrolic ether and distilling at a temperature at which the Water will pass over with the petrolic stantially' as described.

13. In the art of renning-wopl grease, the

method. which consists in saponifying the.

free fatty acids. in the grease, then adding petrolic ether to the mixture of soap and unsaponified grease, and floating'the mixether, subture on water, without agitation, to remove the soap therefrom, substantially as described. i 1

14. In the art of refining wool grease, the method which consists in saponifying the free fatty acids in the rease, then adding petrolic ether to the' mixture of soap and unsaponified grease, and floating the mixture on a Weak salt described. 15. In the art-of refining Wool grease, the method which consists in saponifying the free fatty acids in'the grease, then adding to the mixture. of soap and ,unsaponified grease a solvent which will render the mixsolution, substantially as ture more resistant to subsequent emulsification, thenv floating the mixture on water to remove the soap as described. A

' 16. In the art of refining wool grease, the method which consists in saponifying the free fatty acids in the grease, then holding to the mixture of soap and unsapbnified therefrom, substantially grease a solvent which will render the mixturemore resistant to subsequent emulsifiweak salt solution, substantially 'as descr bed.

in testimony whereof, we. have hereunto set our hands. 4

JAMES O. HANDY. ROBERT M. ISHAM.

Witnesses:

W. C. LYON, H. M. Conwm.

cation, and then floating the mixture on a 

